Construction and Building

Construction and Building Materials 19 (2005) 682690

MATERIALS
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Inuence of coarse aggregate on the permeation, durability and the microstructure characteristics of ordinary Portland cement concrete
L. Basheer *, P.A.M. Basheer, A.E. Long
School of Civil Engineering, Queens University Belfast, Belfast BT7 1NN, Northern Ireland, UK Received 12 February 2005; received in revised form 12 February 2005; accepted 22 February 2005 Available online 26 April 2005

Abstract Reinforced concrete structures in marine and similar environmental conditions have to withstand severe exposures. Due to this, the mix design procedures have to be revised to include durability as a primary criterion along with strength and workability. In line with this need, an investigation was carried out at Queens University Belfast with the nancial help of the Department of Environment, Transport and the Regions, UK. The main objective of the research was to understand the inuence of mix parameters on workability, strength, durability and microstructure and to propose a new mix design procedure within which durability has a higher priority. The present paper reports part of this study, which investigates the eect of size and grading of the coarse aggregate on the durability and the microstructure characteristics of concrete. The durability tests carried out included air permeability test, freeze thaw/salt scaling resistance test and an accelerated carbonation test. The microstructure study was carried out using a scanning electron microscope (SEM) and included image analysis of the interfacial transition zone (ITZ) around the coarse aggregate. The results indicated that as the proportion of larger size aggregate increases in the mix, the local porosity at the ITZ increases and the overall durability decreases. It has also been found that reducing the average aggregate size in a mix improves the pore structure and enhances the durability of the concrete. 2005 Elsevier Ltd. All rights reserved.
Keywords: Concrete; Durability; Microstructure; SEM; ITZ

1. Introduction Most of the important properties of hardened concrete are related to the quantity and characteristics of various types of pores in the cement paste and aggregate components of the concrete. For example, the engineering properties of concrete, such as strength, durability, shrinkage and permeability, are directly inuenced or controlled by the number, type and size of pores present [1]. The total volume of pores, not their size or continuity aect the strength and elasticity of concrete, whereas
*

Corresponding author. Tel.: +28 90974027; fax: +28 90663754. E-mail address: l.basher@qub.ac.uk (L. Basheer).

concrete permeability is inuenced by pore volume, size and continuity. It is believed that capillary voids larger than 50 lm, referred to as macro pores, are detrimental to strength and impermeability, whereas voids smaller than 50 lm, referred to as micro pores, are more related to drying shrinkage and creep [2]. The movement of gases, liquids and ions through concrete is important because of their interactions with concrete constituents and the pore water which can alter the integrity of concrete directly and indirectly, leading to the deterioration of structures. In reinforced concrete this deterioration is mainly due to the corrosion of reinforcement, freezethaw attack or chemical attack. In the recent past the cost of repair of structures due to such

0950-0618/$ - see front matter 2005 Elsevier Ltd. All rights reserved. doi:10.1016/j.conbuildmat.2005.02.022

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deterioration has been high. This has led to eorts by researchers and engineers to understand concrete better so that durable concrete can be produced in the future. Concrete has a highly heterogeneous and complex structure. At the macroscopic level concrete may be considered to be a two-phase material, consisting of aggregate particles dispersed in a matrix of cement paste. At the microscopic level, a third phase the transition zone may be identied (2). This transition zone exists as a thin shell, called the interfacial transition zone (ITZ), between aggregate particles and hydrated cement paste (hcp). It has been established that the ITZ is profoundly dierent from the bulk cement paste in terms of morphology, composition and density [210]. There have been suggestions that the strength of the cement aggregate bond may be the limiting factor in the determination of the ultimate strength of concrete [11]. Furthermore, as the porosity of the ITZ is higher than that of bulk paste [610], the ITZ has a signicant eect on the permeability and durability of concrete. This paper reports a study carried out to ascertain the eect of coarse aggregate grading and size on the permeation properties and durability of concrete. The investigation involved a study of the pore structure characteristics of the ITZ, with the objective of linking the pore structure characteristics to the permeation properties and the durability of ordinary Portland cement concretes. 1.1. Characterisation of interfacial transition zone Back scattered electron (BSE) imaging technique can be used to characterise the pore structure of the ITZ. Low viscosity epoxy impregnated polished samples of concrete are used for BSE imaging. The underlying principle is that the contrast of the BSE images depends on the mean atomic number of the concrete constituents. In the BSE images anhydrous phases of the unreacted cement particles appear bright, the calcium hydroxide light grey, the other hydration products as various shades of darker grey with the epoxy impregnated pores appearing black [8]. Consequently by processing images of polished sections it has been possible to determine the distribution of the phases in hydrated cement paste [12]. Furthermore, these images can also be utilised to ascertain porosity characteristics of the ITZ including the porosity gradient [10] and the amount of penetrable

pores [8,13]. Hence, this technique is used in this work for studying the ITZ pore structure.

2. Experimental programme 2.1. Variables Table 1 gives the mix variables used in the investigation. To obtain a range of coarse aggregate grading the proportion of 10 and 20 mm aggregate was varied. For the aggregate size eect, 10 and 20 mm single size aggregates were used. A constant watercement ratio of 0.6 and aggregatecement ratio of 6 was used in all the cases. Mixes with two dierent ne aggregate-coarse aggregate ratios (FA/CA) were used for both the permeation and durability studies. For the micro structural study only 0.5 FA/CA was used. 2.2. Materials used Class 42.5 N Portland cement [14], medium graded [15] natural sand and crushed basalt coarse aggregate were used for manufacturing the concrete samples. The various properties of the aggregates are summarised in Table 2. To control the moisture condition of the aggregate, all aggregates were oven-dried at a temperature of 40 C. The coarse aggregate was dried for 1 day and the ne aggregate for 2 days. Before the aggregates were used to make concrete they were allowed to cool for at least 1 day. The saturated surface dry 1-hour water absorption values [16] were also measured. This allowed a corrected water quantity to be calculated when batching the materials, to ensure that the aggregate in the concrete was in a saturated surface-dry condition.

Table 2 Properties of aggregates used Aggregate type Fine aggregate (sand) 10 mm crushed basalt 20 mm crushed basalt 1 h absorption (%) 1 0.5 0.5 Specic gravity 2.72 2.93 2.88 Fineness modulus 2.6 5.92 7.04

Table 1 Variable used for the investigation Variable FA/CA Coarse aggregate grading and notation Levels 0.5 100% 10 mm (10 mm) 0.7 67% 10 mm + 33% 20 mm (10/20 = 2) 33% 10 mm + 67% 20 mm (10/20 = 0.5) 100% 20 mm (20 mm)

Note: FA/CA ne aggregatecoarse aggregate ratio.

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2.3. Manufacture of test specimens Six 250 250 100 mm blocks and three 100 mm cubes were cast for each of the variables in Table 1. The blocks were used for the permeation and durability studies and the three cubes were used to obtain the compressive strength (the slump and cube compressive strength values are given in Table 3). One sample from each mix was used for the micro structural study. For each mix the required quantities were batched by mass. These quantities were then mixed together using a pan mixer in accordance with BS 1881: Part 125: 1986 [17]. For both blocks and cubes the concrete was cast in two layers. A vibrating table was used to compact the concrete. Full compaction was considered to have been achieved when air bubbles stopped appearing on the concrete surface. After vibrating, the concrete surface was nished smooth using a metal oat and then covered with a polythene sheet to prevent evaporation of water from the concrete. Approximately, 6 h after the concrete had been cast the moulds were covered with a damp hessian. The moulds were stripped next day and the hardened concrete samples were placed in a constant temperature (20 C) water bath for 3 days. The specimens were then transferred into a storage laboratory kept at a constant temperature of 18 C (2 C) and a relative humidity of 60% ( 5%). When the blocks were 14 days old they were placed in a drying cabinet at a temperature of 40 C and a relative humidity of 20%. This was done to remove moisture from the surface of the concrete in order to eliminate the eect of moisture on the permeation results. After 14 days of drying the specimens were ready for testing. For this they were transferred to a testing laboratory (kept at a constant temperature of 20 C (0.5 C) and relative humidity of 50% ( 5%)) and tested on the following day. The cubes were cured and conditioned in the same way as the slabs in order to ensure that the compressive strength and other parameters were measured using similar concrete. The cubes were then crushed to determine the concrete compressive strength.

2.4. Test methods 2.4.1. Air permeability test The air permeability of concrete was measured on the preconditioned blocks using the Autoclam Permeability system [18]. This test has been used in research for more than a decade and has proved to be very reliable and easy to use. Details of the test can be obtained in [18]. The test provides a relative measure of the air permeability of concrete in Ln(Bar)/min. 2.4.2. Salt scaling test The freezethaw/salt scaling test was carried out according to the RILEM test procedure [19]. The specimens for the test were 100 mm diameter cores taken from the slabs used for the Autoclam air permeability test. The cores were dried for 2 weeks in a fan-assisted cabinet maintained at 40 C and 20% relative humidity. The curved surfaces of these cores were then coated with an epoxy emulsion. These cores were then kept in a 3% sodium chloride solution for 7 days, with the test surface (mould nished face) touching the solution. The face of the cores opposite to the test surface was then coated with the epoxy emulsion. The samples were then transferred to test cells again with the test surface in contact with the 3% salt solution. The cells were then placed in an automatic environmental chamber and subjected to test cycles as shown in Fig. 1. At the end of every two cycles, the specimens were taken out of the chamber and the loose particles removed by means of an ultrasonic bath. The loose particles collected were dried at 100 C for 24 h and then weighed. These measurements were continued for 28 cycles. 2.4.3. Accelerated carbonation test The carbonation resistance of dierent mixes was determined by carrying out an accelerated carbonation test on 100 mm cores removed from the blocks used for the permeability tests. The cores used for the test were dried in a fan-assisted cabinet for 2 weeks at 40 C and 20% relative humidity. These were then coated with epoxy emulsion on the curved surface and the trowel-nished face. When the epoxy was cured,

Table 3 Slump and 28-day compressive strength the study No: 1 2 3 4 5 6 7 8 CA-G 10 mm 10/20 = 2.0 10/20 = 0.5 20 mm 10 mm 10/20 = 2.0 10/20 = 2.0 20 mm FA/CA 0.5 Slump (mm) 35 56 79 103 18 28 23 61 Strength (N/mm2) 46.9 44.1 44.2 42.9 50.1 45.2 45.4 44.9
+20.00 C Time (Hours)

0.00 C

0.7

-20.00C 4.0 Temperature (0 C) 3.0 4.0 1.0

Note: CA-G coarse aggregate grading.

Fig. 1. Freezethaw cycle used for RILEM salt scaling test.

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the cores were placed in an electronically controlled carbonation chamber in an environment of 5 0.1% carbon dioxide at 20 0.5 C and 65 1% relative humidity. At the end of 3 weeks, the samples were taken out and split longitudinally. The freshly broken surface was sprayed with a phenolphthalein indicator solution. After 24 h the depth of the pink coloration was measured to the nearest millimetre at six dierent locations. An average of these values was used for comparing different mixes. 2.4.4. Electron microscopic study of the ITZ Cores of 50 mm diameter were cut from the blocks used for the permeation studies. The cores were then cut along their diameter and a slice of size 25 mm 25 mm 2 mm was removed from the mouldnished face of each core. The slices were then wrapped in thin polythene sheets to prevent any carbonation taking place. These thin slices were dried under vacuum and then impregnated with an ultra low viscosity epoxy. After the epoxy had cured the specimens were polished with diamond grit of progressively ner sizes down to 0.25 lm. The polished samples were then coated with carbon to 10 nm thickness. The carbon-coated samples were placed under a scanning electron microscope (SEM) and 20 backscatter images from around the coarse aggregate present in the slice were collected at random. The image magnication used was 400 times and the electron beam was kept at a distance of 15 mm away from the top of the specimen in all cases. Each image consisted of a small part of aggregate on the left hand side of the picture and the rest was the matrix of cement paste and mortar (Fig. 2(a)). The overall size of each image was 336 262 lm. The porosity gradient was determined using an image analysis computer software programme NIH Image. In order to do this, thresholding of the grey scale to identify pores from the rest was essential. This was done by trial and error and by carrying out a sensitivity analysis. Once the threshold grey scale was decided, the software enabled the determination of porosity in a strip of 10 lm thickness away from the face of the aggregate (Fig. 2(a)). This strip was moved on an incremental basis by 10 lm width away from the face of the coarse aggregate and each time the porosity of the 10 lm thick strip was determined as a percentage of the total area of the strip. Once the strip reached the end of the image, the analysis was repeated on other images collected from the same sample. Therefore, for each 10 lm increment strip away from the coarse aggregate, there were 20 porosity values and an average of these values was reported as the porosity of this 10 lm thick strip of concrete. The average porosity values were then plotted against the distance from the face of the aggregate to determine the characteristics of the interfacial zone (Fig. 2(b)).

Fig. 2. (a) Segmentation using histogram. (b) Typical porosity distribuation curve.

3. Results and discussion 3.1. Slump and compressive strength The slump and 28-day compressive strength results of each mix are presented in Table 3. An increase in slump and marginal decrease in cube compressive strength can be noted with an increase in the proportion of 20 mm aggregate in the mix. The reduction in water demand with an increase in the size of coarse aggregate is well documented [2]. In this experimental programme when the proportion of 20 mm aggregate increased for a given watercement ratio, the reduction in water demand led to the increase in slump. However, as the watercement ratio was not changed, the strength did not vary signicantly. 3.2. Air permeability Tables 4 and 5 give the results of the air permeability test as AP index [18]. When the eect of coarse aggregate grading is considered, it can be seen that as the proportion of 20 mm aggregate increases in the concrete air permeability increases, indicating a reduction in durability [20]. This is seen for both FA/CA ratios. In Table 5,

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Table 4 The eect of aggregate grading on air permeability, salt scaling resistance and carbonation resistance Coarse aggregate grading 10/20 2 10/20 0.5 20 mm 10/20 2 10/20 0.5 20 mm FA/CA 0.5 AP index (Ln(mBar)/min) 0.114 0.139 0.181 0.06 0.105 0.115 Cumulative scaling wt (g) 148.6 406.9 642.3 67.02 53.05 86.05 Depth of carbonation (mm) 12.7 13.1 13.7 12.8 11.3 12.4

0.7

Table 5 The eect of aggregate size on air permeability, salt scaling resistance and carbonation resistance Coarse aggregate size (mm) 10 20 10 20 FA/CA 0.5 0.7 AP index (Ln(mBar)/min) 0.11 0.181 0.076 0.115 Cumulative scaling wt (g) 46.2 642.3 78.05 86.05 Depth of carbonation (mm) 11.1 13.7 11.2 12.4

the eect of increasing the size of coarse aggregate from 10 to 20 mm is to increase the air permeability. There are two possible reasons for these results. When the size of coarse aggregate increases, there is a reduction in the tortuosity of the ow path, which tends to increase the permeability. The second reason is that when larger size coarse aggregates are used, the possibility of the bleed water getting collected below the coarse aggregate increases, which leads to an increase in local watercement ratio and hence the porosity. An increase in porosity around the aggregate would increase the permeability of the concrete. However, Table 6 indicates that only moderate variations in air permeability occurred and all the samples used for this study fall in the region of medium risk concretes in terms of durability [20]. It can also be seen from Tables 4 and 5 that, as the ne aggregatecoarse aggregate ratio was increased from 0.5 to 0.7, the air permeability of the concrete decreased. This is quite unexpected because when the FA/ CA increases, the increase in sand volume for a given aggregatecement ratio would increase the area of interfacial transition zone, which in turn reduce the tortuosity of the ow path. This means that the air permeability should have increased. In Table 3, there is a reduction in slump and an increase in compressive strength with the

increase in FA/CA, which would suggest that when the FA/CA increased, there was an associated decrease in watercement ratio. This might have been the result of increased absorption of mix water by sand over and above that was accounted in mix proportioning. Nevertheless, it can be concluded that the reduction in eective watercement ratio associated with the increase in ne aggregate content is responsible for the reduction in air permeability. Fig. 3 shows the eect of average aggregate size on the air permeability. (The average aggregate size was obtained from the sieve analysis data, using standard procedures). As the average aggregate size in the mix increases the air permeability index increases. A straight line, with a regression coecient of 0.87, can represent this increase. The combined eect of aggregate size, its relative proportion in a mix and the quantity of ne aggregate in the mix on air permeability was obtained by plotting air permeability against the average size of aggregate in Fig. 3. The gure would suggest that the permeability (and hence the durability) of concrete could be improved by reducing the average size of the combined ne and coarse aggregates.

Table 6 Risk rating of durability based on Autoclam air permeability index (20) Air permeability index (Ln(mBar)/min) Range <0.1 0.10.5 0.50.9 >0.9 Rating Low Medium High Very high

0.2 0.18 0.16 0.14 0.12 0.1 0.08 0.06 0.04 0.02 0 0 0.5 1 1.5

AP Index x 102 Ln(Bar)/min

y = 0.0627x - 0.0191 2 R = 0.871

2.5

3.5

Average aggregate size (mm)

Fig. 3. Eect of average aggregate size on air permeablity index.

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n1
porosity % porosity %

n1

n2

(a)

ITZ1 ITZ2 Distance (micron)

(b)

ITZ2 Distance (micron)

Fig. 4. Two dierent types of porosity gradients.

3.3. Salt scaling The salt scaling test gave results similar to those of the air permeability test (Tables 4 and 5). As the proportion of the 20 mm aggregate increases in the mix the cumulative salt scaling also increases, indicating a decrease in durability (Table 4). A similar trend can also be seen in Table 5 when the results of 10 and 20 mm

coarse aggregate mixes are compared for both the FA/ CA ratios. However, the eect of an increase in ne aggregatecoarse aggregate ratio from 0.5 to 0.7 is to improve the salt scaling resistance of the concrete. As in the case of air permeability, it is possible to conclude that an increase in the proportion of smaller size fractions of aggregate in a mix would improve its salt scaling resistance when the watercement ratio is kept constant. However, it has to be pointed out that the eect of the average aggregate size is not as signicant a factor as the watercement ratio of a mix. In a previous study, a lower water cement ratio (0.45) concrete withstood 100 cycles of freezing and thawing [21] compared to 0.6 watercement ratio concrete which only withstood about 28 cycles. 3.4. Carbonation In Table 4, there was no consistent eect of coarse aggregate grading and the FA/CA on the depth of

Fig. 5. (a) Aggregate grading and porosity. (b) Aggregate grading and ITZ thickness. (c) Aggregate grading and total porosity percentage.

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carbonation. Russell and co-workers [22] showed that the depth of carbonation is primarily dependent on the watercement ratio. For the mixes in Table 4, the watercement ratio was kept constant. Therefore, the depth of carbonation remained almost the same for all the mixes. However, Table 5 shows that the depth of carbonation increases when the aggregate size is increased. This is similar to the results reported by Basheer et al. [23]. The increase in the size and porosity of the ITZ around the coarse aggregate due to the increase in size of the coarse aggregate might have contributed to this increase in depth of carbonation. 3.5. ITZ properties The percentage porosity distributions at the ITZ, obtained from SEM analysis, were used for a comparative study of the ITZ in samples from each mix. In general, the distribution of porosity obtained across the ITZ can be divided in to three sections (Fig. 4(a) and (b)):

region of peak porosity (n1) which is about 40 lm thick (ITZ1), a transient porosity region (n2) which is about 160 lm thick (ITZ2), the bulk porosity region (n). The area under the curve in the peak porosity region is termed as A1 and that in the transient porosity region is termed as A2. These values give a combined eect of the percentage porosity and the ITZ. In some cases n2 and the corresponding ITZ1 and A1 values are not present (Fig. 4(b)). Although for microstructure studies in the literature, other researchers have reported the thickness of the ITZ as 1050 lm [8,15,16], a more open approach was used for analysing the results in this paper. This was to avoid losing any valuable information from the results. Fig. 5(a)(c) present the ITZ data versus aggregate grading for mixes of FA/CA ratio 0.5. Results indicate that as the proportion of 20 mm aggregate increases so does the porosity values (n1, n2 and n) (Fig. 5(a)).

Fig. 6. (a) Aggregate size and porosity. (b) Aggregate size and ITZ thickness. (c) Aggregate size and total porosity.

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This eect is more apparent at the ITZ region and is only marginal for the bulk porosity. These result correlate well with the previous three test results given in Sections 3.23.4. When the ITZ thicknesses are compared for these mixes (Fig. 5(b)), it can be seen that as the proportion of 20 mm aggregate increased in the mix, the ITZ thickness also increased. This is more evident in ITZ2 than in ITZ1. Results from this study and a parallel study with dierent watercement ratios and aggregatecement ratios [24] indicate that the ITZ2 value is an important parameter, which has to be considered during the analysis of ITZ results obtained from SEM analysis. From Fig. 5(c) it can be seen that the total porosity percentage, both A1 and A2, increased as the proportion of 20 mm aggregate increased in the mix. Therefore, it can be concluded that when the proportion of course aggregate is increased, there will be an associated increase in interfacial transition zone porosity volume. Fig. 6(a)(c) show the eect of aggregate size on percentage porosity values and ITZ thicknesses. As obtained for the permeation and durability results, reported in Sections 3.23.4, increasing the coarse aggregate size in the mix resulted in an increase in the percentage porosity values (Fig. 6(a)) and the ITZ thicknesses (Fig. 6(b)). These results and the results given in the above paragraphs indicate that the microstructure study using SEM and image analysis give a clear picture of the pore structure distribution at the aggregate interface, which reects the air permeability and durability of the concretes. This is apart from the fact that these images only give a two dimensional picture of the pore structure. Also, there could be error introduced in the SEM analysis because of the fact that it is not known at what angle to the coarse aggregate the concrete was sliced when the samples were prepared. However, Scrivener and Nemati [9] suggest that a correction factor of 0.81 can be applied to the ITZ thickness measured using random sections in order to estimate the average normal distance of the ITZ, provided that sucient number of areas are analysed and averaged [7]. As one sample only was analysed for each variable in this study, this correction factor was not applied.

(ii) Unlike other published work on the eect of ne aggregate content on the air permeability of concrete, when the ne aggregate content increased the air permeability decreased. The increase in tortousity is considered to have contributed to this eect. (iii) The salt scaling resistance followed a trend similar to that of the air permeability reported in (i) and (ii). The eect of aggregate grading and FA/CA on depth of carbonation was insignicant. However, the increase in size of aggregate led to an increase in the depth of carbonation. (iv) The micro structural analysis at the ITZ clearly indicates that the coarser the aggregate the more porous it is at the ITZ. This is in line with the results given by permeability and durability studies. (v) Therefore, in order to design durable concretes using oPc, it is preferable to use smaller size aggregate and a low average aggregate size for the combined ne and coarse aggregate.

Acknowledgements The funding to carryout this project was provided by the Department of Environment, Transport and the Regions, UK. The facilities to carryout this research was provided by the school of Civil Engineering and the Electron microscopic unit at Queens University Belfast. Both these are gratefully acknowledged.

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4. Conclusions On the basis of results presented in this paper, the following conclusions can be drawn: (i) The air permeability of concrete can be improved by resorting to mixes with a low average aggregate size. When the size of coarse aggregate and the proportion of larger size coarse aggregate increases in a mix, there is an associated increase in air permeability.

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